CN104477977A - Method for synthesizing Dy2TiO5 powder by molten-salt growth method - Google Patents

Method for synthesizing Dy2TiO5 powder by molten-salt growth method Download PDF

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CN104477977A
CN104477977A CN201410772948.9A CN201410772948A CN104477977A CN 104477977 A CN104477977 A CN 104477977A CN 201410772948 A CN201410772948 A CN 201410772948A CN 104477977 A CN104477977 A CN 104477977A
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CN104477977B (en
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张玉军
郭学
龚红宇
马丽
张钊
赵新巧
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Shandong University
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    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/003—Titanates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer

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Abstract

The invention relates to a method for synthesizing Dy2TiO5 powder by a molten-salt growth method. The method comprises the following steps: (1) uniformly mixing dysprosium oxide, titanium oxide and alkali metal salt by a ball mill to obtain mixed powder; (2) drying the mixed powder obtained in the step (1) for 6-10h; (3) grinding the material dried in the step (2) and carrying out pre-press forming; (4) warming the material pre-press formed in the step (3) to 800-1400DEG C and preserving the heat to calcine for 1-4h; (5) grinding the material calcined in the step (4), washing by deionized water, filtering, and drying the solid to obtain the Dy2TiO5 powder. According to the preparation method, the Dy2TiO5 powder is synthesized through the molten-salt growth method; compared with a sol-gel process, the preparation method is free of gel process, simple in process, rapid in synthesis speed and low in production cost; the prepared powder is small in grain, uniform in size, good in dispersibility and free of grain adhesion and reunion phenomena.

Description

A kind of molten-salt growth method synthesis Dy 2tiO 5the method of powder
Technical field
The present invention relates to Dy 2tiO 5raw powder's production technology, is specifically related to a kind of molten-salt growth method synthesis Dy 2tiO 5the method of powder, belongs to field of inorganic nonmetallic material.
Background technology
Rare earth titanium hydrochlorate has higher initial neutron absorption ability and unique neutron absorption effectiveness, and have good anti-radiation performance, its fusing point is high, coefficient of thermal expansion is little.In the core industry of present stage, main use is rich in 10the materials such as the norbide of B as command bundle rods for nuclear reactors and shielding protection material, this mainly due to 10b has high thermal neutron absorption cross section, but due to 10can be there is (n, α) reaction in B, produce swelling after being subject to irradiation, affects the stability that it uses, cause shorten its work-ing life; And the lanthanide oxide base ceramic watch of fluorite structure reveals good resistance to radiation damage, wherein with the safe operation in Muscovite MIR reactor of the control rod of metatitanic acid dysprosium ceramic preparation, from nineteen ninety-five, metatitanic acid dysprosium pottery has been applied to Russian VVER-1000 nuclear power generating sets (VD Risovany, EE Varlashova, DN Suslov, Dysprosium titanate as an absorber material for control rods, J.Nucl.Mater., 2000,281:84-89).Metatitanic acid dysprosium pottery has does not release gas and the course of processing does not produce the advantages such as radwaste after neutron radiation, is the extremely potential neutron absorber material of one and command bundle rods for nuclear reactors material.As the Dy preparing high neutron absorption efficiency 2tiO 5the raw material of pottery, Dy 2tiO 5powder should have the features such as high purity, epigranular, favorable dispersity, therefore, and Dy 2tiO 5the preparation research of powder is significant.
The people such as Amit Sinha are with Dy 2o 3, TiO 2for raw material, with MoO 3for stablizer, adopt Solid phase synthesis Dy 2tiO 5powder (Development of dysprosium titanate based ceramics, J.Am.Ceram.Soc., 2005,88 [4]: 1064-1066).The people such as ChoongHwan Jung are with Dy 2o 3, TiO 2for raw material, with MoO 3for stablizer, sol-gel method synthesis technique is adopted to synthesize Dy 2tiO 5powder, (Synthesis and sintering studies on Dy 2tiO 5prepared bypolymer carrier chemical process, J.Nucl.Mater., 2006,354:137-142).But aforesaid method all comes with some shortcomings, such as: in Solid phase synthesis powder process, required calcining temperature is high, and the powder reuniting phenomenon prepared is serious, coarse grains, and sintering activity is low; In sol-gel synthesis powder process, reaction required time is long, and yield poorly, production efficiency is low, in a large amount of preparation process, needs to consume large amount of organic, contaminate environment.
Molten-salt growth method, as preparing oxide ceramic powder body novel process, can reduce synthesis temperature, and Reaction time shorten to a certain extent; In the process of molten-salt growth method synthesizing inorganic powder, fused-salt medium, all the time between the particle of product, prevents between product grain and reunites, and makes the powder of acquisition have good dispersiveness; Molten-salt growth method can control the shape and size of powder crystalline product particle effectively; By changing the kind of fused salt and consumption, the temperature of reaction of system, reaction times and additive add the pattern that effectively can control crystal synthesized by molten-salt growth method.In addition, utilize molten-salt growth method to be conducive to removing the impurity in product, obtain the advantages such as highly purified reaction product has rapidly and efficiently, energy-conserving and environment-protective.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of molten-salt growth method synthesis Dy 2tiO 5the method of powder, the method technique is simple, production cost is low, preparation cycle is short, and obtained product grains size uniform, dispersion effect are good.
Technical solution of the present invention is as follows:
A kind of molten-salt growth method synthesis Dy 2tiO 5the method of powder, with dysprosium oxide, titanium oxide for raw material, be fused-salt medium with an alkali metal salt, the method comprises the following steps:
(1) batch mixing: dysprosium oxide, titanium oxide and an alkali metal salt ball milling are mixed, obtains mixed powder;
Described dysprosium oxide: titanium oxide is 1:(0.8 ~ 1.2 in molar ratio) batching, described an alkali metal salt: the mass ratio of (dysprosium oxide+titanium oxide) is (0.5 ~ 3): 1;
(2) dry: by step (1) gained mixed powder dry 6 ~ 10h at 60 ~ 100 DEG C;
(3) pre-molding: after the material of step (2) dry gained is ground, pre-molding;
(4) calcine: by the material after step (3) pre-molding by the temperature rise rate of 3 ~ 7 DEG C/min from room temperature to 800 DEG C ~ 1400 DEG C, insulation calcining 1 ~ 4h;
(5) washing, drying: the material grinding after step (4) gained is calcined, then use deionized water wash, filter, by solid drying 6 ~ 10h at 60 ~ 100 DEG C, obtain Dy 2tiO 5powder.
According to the present invention, preferably, the dysprosium oxide described in step (1) is Dy 2o 3, described titanium oxide is TiO 2, described an alkali metal salt be NaCl, KCl or/and LiCl, ball-milling medium is dehydrated alcohol;
Preferably, described dysprosium oxide: titanium oxide is 1:1 batching in molar ratio, described an alkali metal salt: the mass ratio of (dysprosium oxide+titanium oxide) is (0.5 ~ 1.5): 1.
According to the present invention, preferably, in step (3), the pressure of pre-molding is 50 ~ 200Mpa.Pre-molding, to keep combining closely between fused salt and raw material, promotes the carrying out of reaction.
According to the present invention, preferably, in step (4), calcining temperature is 1150 ~ 1250 DEG C.
According to the present invention, preferably, supersound process is carried out to material with during deionized water wash in step (5) simultaneously.Supersound process can promote the dissolving of an alkali metal salt, and improves the dispersiveness of powder.
Beneficial effect of the present invention:
1, the present invention synthesizes Dy by molten-salt growth method 2tiO 5powder, compared with sol-gel technology, without the need to gelation process, technique is simple, resultant velocity is fast, production cost is low; Be conducive to the dispersiveness of crystal grain thinning and raising powder; Gained Dy of the present invention 2tiO 5powder median size 2 ~ 3 μm.
2, the present invention adopts molten-salt growth method, can reuse, reduce production cost after fused salt cleaning, and obtained powder grain is little, size uniform, good dispersity, without crystal grain adhesion agglomeration.
Accompanying drawing explanation
The X ray diffracting spectrum of the sample of Fig. 1 obtained by the embodiment of the present invention 1.
The SEM photo of the sample of Fig. 2 obtained by the embodiment of the present invention 1.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described further, but institute of the present invention protection domain is not limited thereto.
Raw materials usedly in embodiment be convenient source, equipment used is conventional equipment, commercial products.
In embodiment, ball-milling medium is dehydrated alcohol.
Embodiment 1:
A kind of molten-salt growth method synthesis Dy 2tiO 5the method of powder, step is as follows:
(1) batch mixing: take 41g Dy 2o 3, 9g TiO 2, 75gNaCl, by Dy 2o 3, TiO 2be placed in high-speed mixing ball mill with NaCl to mix, obtain mixed powder; Dy in powder 2o 3: TiO 2mol ratio is 1:1, NaCl quality and Dy 2o 3, TiO 2total mass ratio is 1.5:1;
(2) dry: mixed powder described in step (1) to be placed in convection oven, forced air drying 10h at 80 DEG C;
(3) pre-molding: the material of step (2) dry gained is placed in mortar, after grinding, pre-molding under pressure is 50MPa;
(4) calcine: the material after step (3) pre-molding is placed in box-type furnace, with the temperature rise rate of 5 DEG C/min from room temperature to 1200 DEG C, insulation calcining 1h;
(5) washing, drying: the material after being calcined by step (4) gained grinds, powder after grinding in ultrasonic machine with after deionized water wash, supernatant liquor removes by standing or suction filtration, after carrying out 3 ~ 5 washings, be placed in convection oven, at 80 DEG C, forced air drying 10h, obtains Dy 2tiO 5powder.
The Dy that the present embodiment is prepared 2tiO 5powder test X ray diffracting spectrum and SEM photo, as shown in Figure 1, 2.
As shown in Figure 1, the powder product obtained is Dy 2tiO 5powder.As shown in Figure 2, the Dy obtained 2tiO 5the median size of powder about 2 ~ 3 μm, even particle size distribution, good dispersity, without crystal grain adhesion agglomeration.
Embodiment 2:
A kind of molten-salt growth method synthesis Dy 2tiO 5the method of powder, step is as follows:
(1) batch mixing: take 41g Dy 2o 3, 9g TiO 2, 100gNaCl, by Dy 2o 3, TiO 2be placed in high-speed mixing ball mill with NaCl to mix, obtain mixed powder; Dy in powder 2o 3: TiO 2mol ratio is 1:1, NaCl quality and Dy 2o 3, TiO 2total mass ratio is the raw material of 2:1;
(2) dry: mixed powder described in step (1) to be placed in convection oven, forced air drying 10h at 80 DEG C;
(3) pre-molding: dry for step (2) gained material is placed in mortar, after grinding, pre-molding under pressure is 150MPa;
(4) calcine: the material after step (3) pre-molding is placed in box-type furnace, with the temperature rise rate of 5 DEG C/min from room temperature to 1150 DEG C, insulation calcining 2h;
(5) washing, drying: the material after being calcined by step (4) gained grinds, powder after grinding in ultrasonic machine with after deionized water wash, supernatant liquor removes by standing or suction filtration, after carrying out 3 ~ 5 washings, be placed in convection oven, at 80 DEG C, forced air drying 10h, obtains Dy 2tiO 5powder.
Embodiment 3:
A kind of molten-salt growth method synthesis Dy 2tiO 5the method of powder, step is as follows:
(1) batch mixing: take 41g Dy 2o 3, 9g TiO 2, 50g KCl, by Dy 2o 3, TiO 2be placed in high-speed mixing ball mill with KCl to mix, obtain mixed powder; Dy in powder 2o 3: TiO 2mol ratio is 1:1, KCl quality and Dy 2o 3, TiO 2total mass ratio is the raw material of 1:1;
(2) dry: mixed powder described in step (1) to be placed in convection oven, forced air drying 10h at 80 DEG C;
(3) pre-molding: the material of step (2) dry gained is placed in mortar, after grinding, pre-molding under pressure is 100MPa;
(4) calcine: the material after step (3) pre-molding is placed in box-type furnace, with the temperature rise rate of 5 DEG C/min from room temperature to 1250 DEG C, insulation calcining 2h;
(5) washing, drying: the material after being calcined by step (4) gained grinds, powder after grinding in ultrasonic machine with after deionized water wash, supernatant liquor removes by standing or suction filtration, after carrying out 3 ~ 5 washings, be placed in convection oven, at 80 DEG C, forced air drying 10h, obtains Dy 2tiO 5powder.
Embodiment 4:
A kind of molten-salt growth method synthesis Dy 2tiO 5the method of powder, step is as follows:
(1) batch mixing: take 41g Dy 2o 3, 9g TiO 2, 50g LiCl, by Dy 2o 3, TiO 2be placed in high-speed mixing ball mill with LiCl to mix, obtain mixed powder; Dy in powder 2o 3: TiO 2mol ratio is 1:1, LiCl quality and Dy 2o 3, TiO 2total mass ratio is the raw material of 1:1;
(2) dry: mixed powder described in step (1) to be placed in convection oven, forced air drying 10h at 80 DEG C;
(3) pre-molding: dry for step (2) gained material is placed in mortar, after grinding, pre-molding under pressure is 150MPa;
(4) calcine: the material after step (3) pre-molding is placed in box-type furnace, with the temperature rise rate of 3 DEG C/min from room temperature to 1250 DEG C, insulation calcining 2h;
(5) washing, drying: the material after being calcined by step (4) gained grinds, powder after grinding in ultrasonic machine with after deionized water wash, supernatant liquor removes by standing or suction filtration, after carrying out 3 ~ 5 washings, gained powder is placed in convection oven, at 80 DEG C, forced air drying 10h, obtains Dy 2tiO 5powder.
Embodiment 5:
A kind of molten-salt growth method synthesis Dy 2tiO 5the method of powder, step is as follows:
(1) batch mixing: take 41g Dy 2o 3, 9g TiO 2, 100g NaCl-KCl, NaCl-KCl mass ratio is 1:1, by Dy 2o 3, TiO 2be placed in high-speed mixing ball mill with NaCl-KCl to mix, obtain mixed powder; Dy in powder 2o 3: TiO 2mol ratio is 1:1, NaCl-KCl quality and Dy 2o 3, TiO 2total mass ratio is the raw material of 2:1;
(2) dry: mixed powder described in step (1) to be placed in convection oven, forced air drying 10h at 80 DEG C;
(3) pre-molding: the material of step (2) dry gained is placed in mortar, after grinding, pre-molding under pressure is 150MPa;
(4) calcine: the material after step (3) pre-molding is placed in box-type furnace, with the temperature rise rate of 5 DEG C/min from room temperature to 1250 DEG C, insulation calcining 2h;
(5) washing, drying: the material after being calcined by step (4) gained grinds, powder after grinding in ultrasonic machine with after deionized water wash, supernatant liquor removes by standing or suction filtration, after carrying out 3 ~ 5 washings, gained powder is placed in convection oven, at 80 DEG C, forced air drying 10h, obtains Dy 2tiO 5powder.
It should be noted that, what more than enumerate is only several specific embodiments of the present invention, and obvious the present invention is not limited only to above embodiment, and other can also be had to be out of shape.All distortion that those skilled in the art directly derives from the disclosure of invention or indirectly amplifies, all should think protection scope of the present invention.

Claims (7)

1. a molten-salt growth method synthesis Dy 2tiO 5the method of powder, with dysprosium oxide, titanium oxide for raw material, be fused-salt medium with an alkali metal salt, the method comprises the following steps:
(1) batch mixing: dysprosium oxide, titanium oxide and an alkali metal salt ball milling are mixed, obtains mixed powder;
Described dysprosium oxide: titanium oxide is 1:(0.8 ~ 1.2 in molar ratio) batching, described an alkali metal salt: the mass ratio of (dysprosium oxide+titanium oxide) is (0.5 ~ 3): 1;
(2) dry: by step (1) gained mixed powder dry 6 ~ 10h at 60 ~ 100 DEG C;
(3) pre-molding: after the material of step (2) dry gained is ground, pre-molding;
(4) calcine: by the material after step (3) pre-molding by the temperature rise rate of 3 ~ 7 DEG C/min from room temperature to 800 DEG C ~ 1400 DEG C, insulation calcining 1 ~ 4h;
(5) washing, drying: the material grinding after step (4) gained is calcined, then use deionized water wash, filter, by solid drying 6 ~ 10h at 60 ~ 100 DEG C, obtain Dy 2tiO 5powder.
2. molten-salt growth method synthesis Dy according to claim 1 2tiO 5the method of powder, is characterized in that, the dysprosium oxide described in step (1) is Dy 2o 3, described titanium oxide is TiO 2, described an alkali metal salt is that NaCl, KCl are or/and LiCl.
3. molten-salt growth method synthesis Dy according to claim 1 2tiO 5the method of powder, is characterized in that, dysprosium oxide described in step (1): titanium oxide is 1:1 batching in molar ratio.
4. molten-salt growth method synthesis Dy according to claim 1 2tiO 5the method of powder, is characterized in that, an alkali metal salt described in step (1): the mass ratio of (dysprosium oxide+titanium oxide) is (0.5 ~ 1.5): 1.
5. molten-salt growth method synthesis Dy according to claim 1 2tiO 5the method of powder, is characterized in that, in step (3), the pressure of pre-molding is 50 ~ 200Mpa.
6. molten-salt growth method synthesis Dy according to claim 1 2tiO 5the method of powder, is characterized in that, in step (4), calcining temperature is 1150 ~ 1250 DEG C.
7. molten-salt growth method synthesis Dy according to claim 1 2tiO 5the method of powder, is characterized in that, carries out supersound process in step (5) with during deionized water wash to material simultaneously.
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Cited By (5)

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CN105161144A (en) * 2015-08-07 2015-12-16 厦门大学 Preparation method of dysprosium titanium oxide pellet serving as neutron absorbing material of nuclear reactor core
CN107572573A (en) * 2017-10-26 2018-01-12 贵州大学 A kind of preparation method of the nano ceric oxide particle of polyhedral structure
CN107601546A (en) * 2017-10-26 2018-01-19 贵州大学 A kind of environment-friendly preparation method thereof of nano ceric oxide particle
CN112340777A (en) * 2020-10-30 2021-02-09 中科立民新材料（扬州）有限公司 Method for synthesizing pure lanthanum chromate at low temperature, lanthanum chromate synthesized by method and application of lanthanum chromate
CN113213916A (en) * 2021-05-19 2021-08-06 山东大学 Fluorite-structured dysprosium titanate reactor control rod and preparation method thereof

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CN102701273A (en) * 2012-05-22 2012-10-03 山东大学 Preparation method of nano dysprosium titanate powder

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105161144A (en) * 2015-08-07 2015-12-16 厦门大学 Preparation method of dysprosium titanium oxide pellet serving as neutron absorbing material of nuclear reactor core
CN105161144B (en) * 2015-08-07 2017-09-08 厦门大学 A kind of preparation method of nuclear reactor neutron absorber material metatitanic acid dysprosium pellet
CN107572573A (en) * 2017-10-26 2018-01-12 贵州大学 A kind of preparation method of the nano ceric oxide particle of polyhedral structure
CN107601546A (en) * 2017-10-26 2018-01-19 贵州大学 A kind of environment-friendly preparation method thereof of nano ceric oxide particle
CN112340777A (en) * 2020-10-30 2021-02-09 中科立民新材料（扬州）有限公司 Method for synthesizing pure lanthanum chromate at low temperature, lanthanum chromate synthesized by method and application of lanthanum chromate
CN113213916A (en) * 2021-05-19 2021-08-06 山东大学 Fluorite-structured dysprosium titanate reactor control rod and preparation method thereof
CN113213916B (en) * 2021-05-19 2022-02-11 山东大学 Fluorite-structured dysprosium titanate reactor control rod and preparation method thereof

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